CN102250400A - Polymer matrix composite material with high PTC strength and stability and preparation method thereof - Google Patents
Polymer matrix composite material with high PTC strength and stability and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polymer matrix composite material with high PTC strength and stability and a preparation method thereof, and the composite material comprises UHMWPE and PVDF, CB and MWNT conductive filling materials which are treated by surface treatment by a titanate coupling agent, and an antioxidant 1010; the preparation method comprises the following steps: performing surface treatment of the CB and MWNT conductive filling materials by the titanate coupling agent, performing vacuum drying of PVDF and UHMWPE with a volume ratio of 1:1, adding PVDF into a torque rheometer, heating and melting for 2 min, adding another matrix of UHMWPE and the antioxidant 1010, wherein the amount of the antioxidant 1010 is 1% of the total mass of the matrix; mixing the mixture of the two matrixes for 10 min, adding the filling materials, mixing at 250 DEG C for 15 min; after melt blending, performing hot pressing with a constant temperature of 250 DEG C and a constant pressure of 18 MPa for 10 min to obtain the sample. The composite material of the invention has good conductivity and low room-temperature conductivity, and has a conductivity of up to 10-1 near a percolation threshold; the conductivity of the composite material can be changed by adjusting the contents of the filling materials in the composite material; the composite material has high PTC strength, good repetition stability, and reduced NTC effect.
Description
Technical field
The invention belongs to the polymer matrix PTC matrix material of hyundai electronics and the widespread use of electric works field, a kind of PTC matrix material of particularly high PTC intensity, good cyclicity and stability and preparation method thereof.
Background technology
Polymer matrix PTC material is a body material with single component crystallization or semi-crystalline polymer mainly at present, is conductive filler material with the high graphitized carbon black of cost performance (CB).Along with making rapid progress of modern science and technology, the polymer matrix PTC material Application Areas is constantly expanded, the polymer matrix PTC material of single structure has been difficult to satisfy needs of society, and material is difficult to realize the control of material structure and differentiation, cause the electric heating property of polymer PTC product stable inadequately, the function of related electronic devices is difficult to realize.The problem that exists mainly is that room temperature resistivity is higher, and cyclical stability is poor, and abroad in theoretical and the technical a certain distance that exists.Therefore, the polymer matrix composite that over-all properties is better is an at present domestic and international ten minutes active subject.Multi-walled carbon nano-tubes (MWNT) and CB particle with certain length-to-diameter ratio are filled out two-component polymer altogether, can further improve material PTC effect: lower seepage flow threshold value and room temperature resistivity, high PTC intensity, good cyclical stability.
Summary of the invention
The purpose of this invention is to provide polymer matrix composite of a kind of high PTC intensity and stability and preparation method thereof.
The present invention is the polymer matrix composite of a kind of high PTC intensity and stability, comprises in the matrix material: polymer matrix material ultra-high molecular weight (5,000,000 grades of molecular weight) polyethylene (UHMWPE) and polyvinylidene difluoride (PVDF) (PVDF), titanate coupling agent surface-treated CB and MWNT conductive filler material and antioxidant 1010; The volume ratio of described polymer matrix material UHMWPE and PVDF is 1: 1, described CB particle accounts for 4.0% of filler and polymer matrix material cumulative volume, the volume fraction that the MWNT conductive filler material accounts for cumulative volume is 0-3%, and antioxidant 1010 is 1% of a matrix total mass; Diameter 10～the 30nm of multi-walled carbon nano-tubes (MWNT), length 5～15 μ m.
The preparation of matrix material may further comprise the steps:
(1) surface treatment of CB: in order to improve the dispersiveness of CB in matrix material, adopting titanate coupling agent (NDZ-102) that it is carried out early stage handles, CB is all put into the ethanolic soln of titanate coupling agent, behind the ball milling 2h in baking oven evaporating solvent, place then under 120 ℃ of conditions of vacuum drying oven and react 1h, obtain modification CB, wherein the mass ratio of titanate coupling agent and CB is 1: 100;
(2) surface treatment of MWNT: the ethanolic soln of MWNT being put into titanate coupling agent, behind the ultrasonication 2h in baking oven evaporating solvent, place then under 120 ℃ of conditions of vacuum drying oven and react 1h, obtain the MWNT of modification, wherein the mass ratio of titanate coupling agent and MWNT is 1: 100;
(3) compound: by PVDF and UHMWPE volume ratio is to take by weighing PVDF and UHMWPE at 1: 1, and takes by weighing step (1), and CB and MWNT that (2) modification obtains make CB account for filler and the matrix total volume fraction is 4%, and the volume fraction that MWNT accounts for cumulative volume is 0-3%; Matrix at first joins PVDF in the torque rheometer through after the vacuum-drying, and the adjustment rotating speed is 50r/min, allows its heating and melting 2 minutes, adds another matrix UHMWPE and antioxidant 1010 then, and antioxidant 1010 is 1% of a matrix total mass; With mixing 10 minutes of the mixture of two kinds of matrixes, add filler then, 250 ℃ are mixing 15 minutes; After melt blending is finished, discharging; (4) moulding: 250 ℃, 18MPa constant temperature and pressure hot pressing 10 minutes promptly obtains sample.
The present invention has following beneficial effect:
1. in matrix material, have dispersed preferably with CB after titanate coupling agent (NDZ-102) modification and MWNT.
2. fill out altogether by the single filler of interpolation or two kinds of dissimilar fillers in mutual exclusive pair of component matrix, the polymer matrix PTC material through the preparation of melt blending compounding technology has significant PTC performance: high PTC intensity and good repetition stability.
3. adopt mutual exclusive two-phase matrix to make matrix material the seepage flow phenomenon to occur than low sizing content the time, have electroconductibility and lower room-temperature conductivity preferably, specific conductivity reaches 10 near the seepage flow threshold value
-1, can change the electroconductibility of matrix material by the content of regulating filler in the matrix material.
4. by adding MWNT as second filler, make the viscosity of system increase, owing to the synergy between MWNT and CB long-range conduction and the short range conduction, the reunion movability of conductive filler material reduces simultaneously, thereby obtain high PTC intensity and good repetition stability, the NTC effect reduces.
Description of drawings
The profile scanning electromicroscopic photograph of Fig. 1 embodiment 1 matrix material;
The profile scanning electromicroscopic photograph of Fig. 2 embodiment 2 matrix materials;
The conductivity at room temperature performance of Fig. 3 embodiment 1 and Comparative Examples matrix material and seepage flow threshold value;
Wherein the A-example 1; The B-Comparative Examples
Fig. 4 adds the PTC performance study of the matrix material of different volumes mark MWNT;
A-example 1; B-example 2; C-example 3; D-example 4
Fig. 5 MWNTf
MWNTThe PTC repetitive research of=1% matrix material;
Fig. 6 MWNTf
MWNTThe PTC repetitive research of=2% matrix material;
Fig. 7 f
MWNTPTC performance study in=0 matrix material heating and cooling process;
Fig. 8 f
MWNTPTC performance study in=1% matrix material heating and cooling process.
Specific implementation method:
Example 1
(1) the 0.06g titanate coupling agent is dissolved in the 50ml ethanol, magnetic agitation is fully diluted evenly it.6gCB is put into titanate coupling agent solution, use the coupling agent modified of massfraction 1%, ball milling 2h puts into 120 ℃ of following evaporating solvents of baking oven then.CB after the oven dry places vacuum drying oven, and 120 ℃ vacuumize constant temperature 1h, it is fully reacted and drying, obtains needed surface-functionalized CB;
(2) be respectively to take by weighing 34.37gPVDF, 17.95gUHMWPE, CB (f that 2.98g step (1) obtain at 1: 1 by PVDF and PP volume ratio
CB=4%) and the 0.52g antioxidant 1010.In the Hakke torque rheometer, at first, heating and melting PVDF 2 minutes; Add UHMWPE and antioxidant 1010 then.With mixing 10 minutes of the mixture of two kinds of matrixes; Add CB then, 250 ℃ mixing 15 minutes in batches; After melt blending is finished, discharging;
(3) matrix material that step (2) is obtained is at 250 ℃, and constant temperature and pressure is 10 minutes under the 18MPa condition, and naturally cooling is pressed into thick 1mm, (PVDF/UHMWPE) (CB-filled-(PVDF/UHMWPE)) (f that the CB of diameter 12mm fills
CB=4%) disk sample;
(4) starch in 100 ℃ of processing 2h at the sample two ends coated with conductive silver that step (3) obtains, 24h is stablized in the cooling cooling naturally, and material is well contacted with the silver slurry, reduces the contact resistance in the test process.Profile scanning electromicroscopic photograph such as Fig. 1 of matrix material, conductivity under the room temperature and seepage flow threshold value shown in Fig. 3-B, PTC performance such as Fig. 4-A, PTC performance such as Fig. 7 in the heating and cooling process.
By Fig. 1, CB is evenly distributed in matrices of composite material.
Comparative Examples
(1) CB particulate process of surface treatment is with example 1.
(2) by taking by weighing 68.74gPVDF, the CB (f that 2.98g step (1) obtains
CB=4%) and the 0.68g antioxidant 1010.In the Hakke torque rheometer, at first, heating and melting PVDF and antioxidant 1010 add CB then in batches, and 250 ℃ mixing 15 minutes; After melt blending is finished, discharging;
(3) matrix material that step (2) is obtained is at 250 ℃, and constant temperature and pressure is 10 minutes under the 18MPa condition, and naturally cooling is pressed into thick 1mm, (PVDF that CB fills) CB-filled-PVDF (f of diameter 12mm
CB=4%) disk sample;
(4) starch in 100 ℃ of processing 2h at the sample two ends coated with conductive silver that step (3) obtains, 24h is stablized in the cooling cooling naturally, and material is well contacted with the silver slurry, reduces the contact resistance in the test process.Conductivity under the room temperature of matrix material and seepage flow threshold value are shown in Fig. 3-A.
Curve A and B in the comparison diagram 3, behind the adding UHMWPE, the seepage flow threshold value reduces greatly in the matrix material.
Example 2
(1) CB particulate process of surface treatment is with example 1.
(2) the 0.06g titanate coupling agent is dissolved in the 50ml ethanol, magnetic agitation is fully diluted evenly it.6gCB is put into titanate coupling agent solution, and ultra-sonic dispersion 2h puts into 120 ℃ of following evaporating solvents of baking oven then.MWNT after the oven dry places vacuum drying oven, and 120 ℃ vacuumize constant temperature 1h, it is fully reacted and drying, obtains needed surface-functionalized MWNT;
(2) be respectively to take by weighing 34gPVDF, 17.77gUHMWPE, 0.52g antioxidant 1010, CB (f that 2.98g step (1) obtain at 1: 1 by PVDF and PP volume ratio
CB=4%), and the MWNT (f that obtains of 0.75g step (2)
MWNT=1%).In the Hakke torque rheometer, at first, heating and melting PVDF 2 minutes; Add UHMWPE and antioxidant 1010 then, with mixing 10 minutes of the mixture of two kinds of matrixes; Add CB and MWNT then, 250 ℃ mixing 15 minutes in batches; After melt blending is finished, discharging;
(3) matrix material that step (2) is obtained is on thermocompressor 250 ℃, constant temperature and pressure is 10 minutes under the 18MPa condition, naturally cooling is pressed into thick 1mm, (PVDF/UHMWPE) ((MWNT/CB)-co-filled-(PVDF/UHMWPE)) (f that (MWNT/CB) of diameter 12mm fills altogether
CB=4%, f
MWNT=1%) disk sample;
(4) starch in 100 ℃ of processing 1h at the sample two ends coated with conductive silver that step (3) obtains, naturally 24h is stablized in the cooling back, material is well contacted with the silver slurry, reduce the contact resistance in the test process, profile scanning electromicroscopic photograph such as Fig. 2 of matrix material, PTC performance such as Fig. 4-B, PTC is repeated as Fig. 5, PTC performance such as Fig. 8 in the heating and cooling process.
As Fig. 2, MWNT has played certain " bridge joint " effect in matrix material.Can get from Fig. 5, PTC has better repeatability behind the adding MWNT.Comparison diagram 7 and 8 gets, and the resistance temperature of matrix material in heating and cooling process returned to stagnate to enclose and diminished behind the adding MWNT, and just PTC repeatability improves.
Example 3
(1) CB particulate process of surface treatment is with example 1, and the process of surface treatment of MWNT is with example 2.
(2) be respectively to take by weighing 33.65g PVDF, 17.58g UHMWPE, CB (f that 0.51g antioxidant 1010 and 2.98g step (1) obtain at 1: 1 by PVDF and PP volume ratio
CB=4%), and the MWNT (f that obtains of 1.50g step (2)
MWNT=2%).In the Hakke torque rheometer, at first, heating and melting PVDF 2 minutes; Add UHMWPE and antioxidant 1010 then, with mixing 10 minutes of the mixture of two kinds of matrixes; Add CB and MWNT then, 250 ℃ mixing 15 minutes in batches; After melt blending is finished, discharging;
(3) matrix material that step (2) is obtained is on thermocompressor 250 ℃, constant temperature and pressure is 10 minutes under the 18MPa condition, naturally cooling is pressed into thick 1mm, (PVDF/UHMWPE) ((MWNT/CB)-co-filled-(PVDF/UHMWPE)) (f that (MWNT/CB) of diameter 12mm fills altogether
CB=4%, f
MWNT=2%) disk sample;
(4) starch in 100 ℃ of processing 1h at the sample two ends coated with conductive silver that step (3) obtains, naturally 24h is stablized in the cooling back, and material is well contacted with the silver slurry, reduces the contact resistance in the test process, the PTC performance of matrix material as shown in Figure 4, PTC repeatability is as Fig. 6.
Example 4
(1) CB particulate process of surface treatment is with example 1, and the process of surface treatment of MWNT is with example 2.
(2) be respectively to take by weighing 33.29g PVDF, 17.39g UHMWPE, 0.5g antioxidant 1010, CB (f that 2.98g step (1) obtain at 1: 1 by PVDF and PP volume ratio
CB=4%), and the MWNT (f that obtains of 2.25g step (2)
MWNT=3%).In the Hakke torque rheometer, at first, heating and melting PVDF 2 minutes; Add UHMWPE and antioxidant 1010 then, with mixing 10 minutes of the mixture of two kinds of matrixes; Add CB and MWNT then, 250 ℃ mixing 15 minutes in batches; After melt blending is finished, discharging;
(3) matrix material that step (2) is obtained is on thermocompressor 250 ℃, constant temperature and pressure is 10 minutes under the 18MPa condition, naturally cooling is pressed into thick 1mm, (PVDF/UHMWPE) ((MWNT/CB)-co-filled-(PVDF/UHMWPE)) (f that (MWNT/CB) of diameter 12mm fills altogether
CB=4%, f
MWNT=3%) disk sample;
(4) starch in 100 ℃ of processing 1h at the sample two ends coated with conductive silver that step (3) obtains, 24h is stablized in the cooling back naturally, and material is well contacted with the silver slurry, reduces the contact resistance in the test process, and the PTC performance of matrix material as shown in Figure 4.
A, B, four curves of C, D can get in the comparison diagram 4, and the PTC intensity of matrix material can improve after adding a certain amount of MWNT in the system, but add-on is excessive, can make PTC intensity reduce on the contrary, and promptly the add-on of MWNT has an optimum value.
Claims (3)
1. the polymer matrix composite of one kind high PTC intensity and stability, it is characterized in that, comprise in the matrix material: polymer matrix material ultrahigh molecular weight polyethylene(UHMWPE) (UHMWPE) and polyvinylidene difluoride (PVDF) (PVDF), titanate coupling agent surface-treated CB and MWNT conductive filler material and antioxidant 1010; The volume ratio of described polymer matrix material UHMWPE and PVDF is 1: 1, described CB particle accounts for 4.0% of filler and polymer matrix material cumulative volume, the volume fraction that the MWNT conductive filler material accounts for cumulative volume is 0-3%, and antioxidant 1010 is 1% of a matrix total mass.
2. according to the polymer matrix composite of claim 1, it is characterized in that the diameter 10～30nm of described multi-walled carbon nano-tubes (MWNT), length 5～15 μ m.
3. the preparation method of the polymer matrix composite of the high PTC intensity of claim 1 and stability is characterized in that, may further comprise the steps:
(1) surface treatment of CB: in order to improve the dispersiveness of CB in matrix material, adopting titanate coupling agent (NDZ-102) that it is carried out early stage handles, CB is all put into the ethanolic soln of titanate coupling agent, behind the ball milling 2h in baking oven evaporating solvent, place then under 120 ℃ of conditions of vacuum drying oven and react 1h, obtain modification CB, wherein the mass ratio of titanate coupling agent and CB is 1: 100;
(2) surface treatment of MWNT: the ethanolic soln of MWNT being put into titanate coupling agent, behind the ultrasonication 2h in baking oven evaporating solvent, place then under 120 ℃ of conditions of vacuum drying oven and react 1h, obtain the MWNT of modification, wherein the mass ratio of titanate coupling agent and MWNT is 1: 100;
(3) compound: by PVDF and UHMWPE volume ratio is to take by weighing PVDF and UHMWPE at 1: 1, and takes by weighing step (1), and CB and MWNT that (2) modification obtains make CB account for filler and the matrix total volume fraction is 4%, and the volume fraction that MWNT accounts for cumulative volume is 0-3%; Matrix at first joins PVDF in the torque rheometer through after the vacuum-drying, and the adjustment rotating speed is 50r/min, allows its heating and melting 2 minutes, adds another matrix UHMWPE and antioxidant 1010 then, and antioxidant 1010 is 1% of a matrix total mass; With mixing 10 minutes of the mixture of two kinds of matrixes, add filler then, 250 ℃ are mixing 15 minutes; After melt blending is finished, discharging;
(4) moulding: 250 ℃, 18MPa constant temperature and pressure hot pressing 10 minutes promptly obtains sample.
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| CN103483666A (en) * | 2013-09-29 | 2014-01-01 | 太仓金凯特种线缆有限公司 | Method for preparing PTC (positive temperature coefficient) material by compounding polyaniline/carbon black/polyolefin |
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| US20050070658A1 (en) * | 2003-09-30 | 2005-03-31 | Soumyadeb Ghosh | Electrically conductive compositions, methods of manufacture thereof and articles derived from such compositions |
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| US20050070658A1 (en) * | 2003-09-30 | 2005-03-31 | Soumyadeb Ghosh | Electrically conductive compositions, methods of manufacture thereof and articles derived from such compositions |
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| CN103483666A (en) * | 2013-09-29 | 2014-01-01 | 太仓金凯特种线缆有限公司 | Method for preparing PTC (positive temperature coefficient) material by compounding polyaniline/carbon black/polyolefin |
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